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The decarboxylative acetoxylation of carboxylic acids using a combination of PhI(OAc) 2 and I 2 in a CH 2 Cl 2 /AcOH mixed solvent is reported. The reaction was successfully applied to two types of carboxylic acids containing an α-quaternary and a benzylic carbon center under mild reaction conditions. The resulting acetates were readily converted into the corresponding alcohols by hydrolysis.

Hypervalent iodine(III)-mediated decarboxylative acetoxylation at tertiary and benzylic carbon centers